Processes for incorporating encapsulated flavors and the like in reconstituted tobacco sheet



United States Patent n 11 3,540,456

[72] Inventors James H. lgcGltitmphy [56] References Cited Chflham, WUNITED STATES PATENTS James Orville Pfaif, New York, New York; 3 006 34710/196] Keam I3 1 l5 Alton De Witt Quinn, Craniord, New n I JerseyGeorges weumr New York New 3,106,211 /1963 Reynolds et a1. 131/1-7 York3,334,636 8/1967 Zuber 131/10.1 pp No 844,233 3,339,558 9/1967 Waterbury131/101 221 Filed May 29, 1969 FOREIGN PATENTS Division of Ser. No.660,775, Aug. 15, 1967 188,572 3/1964 Sweden 131/ 10.1 Patented [970Primar Examiner-Melvin D. Rein [73] Assignee glgggtigmlCash RegisterCompany Frank McKinhey D a corporation of Maryland ABST RACT: Theformation of reconstituted tobacco sheet PROCESSES FOR INCORPORATINGmaterial from tobacco stems, said sheet havmg a subsident ENCAPSULATEDFLAVORS AND THE LIKE IN layer of microencapsulated flavoring materialembedded in RECONSTITUTED TOBACCO SHEET the reconstituted tobacco sheetand the incorporation thereof 2 Cl 6 D F into smoking articles such ascigarettes, cigars, etc.

rawmg The microcapsules are of an average diameter smaller than [52],US. Cl 131/144, the sheet thickness and in such quantity as to beconfined '131/10.1,13l/140 within the sheet, being protectively nestedin the spaces [51] Int. Cl A241) 3/14; between the tobacco fibers. Theyare incorporated within an A24d 1/06 aqueous tobacco slurry beforesheeting or applied to a wet Field ofSearch 131/ 10.1,9, web of fibroustobacco on a support in a suspension which contains a film formingpolymeric material.

Patented Nev. 17, 1970 FIG. 3

FIG, 6

FIG.

INVENTORS JAMES H, MCGLUMPHY JAMES O. PFAFF ALTON D. QUINN 8 GEORGEWELLNER FLAYORS AND THE LIKE IN RECONSTITUTED TOBACCO SHEET This is adivision of U.S. Pat. application Ser. No. 660,775, filed Aug. I5, 1967.

This invention relates to an improvement in reconstituted tobaccoprocessing whereby a plurality of minute, heat rupturable capsules eachcontaining an aromatic substance such as menthol as an inner phase aremixed in integral contiguous relationship with tobacco. As tobaccosurrounding each discrete capsule burns, the elevation in temperature issuch that capsule walls rupture, therebyreleasing a discrete quantity ofaromatic substance which becomes entrained in smoke issuing from theburning tobacco. The capsules being spaced homogeneously throughout thelength of the smoking article, the capsule walls rupture successively.or consecutively, with the advance of the burning front of ignitedtobacco. The exeunt smoke inhaled by the smoker is homogeneouslyaromatic. I

This invention relates to methods for producing reconstituted sheet orfilm material having capsules contained therein ofencapsulated flavoringmaterial.

This invention relates to a system for providing a subsident layer ofmicrocapsules containing flavoring material in reconstituted fibroustobacco sheets; and to the novel product produced thereby.

The present invention can be practiced by spraying a capsule slurry ontoreconstituted tobacco sheet material or film made from a selectedportion of the stems of tobacco. It has been found that although tobaccostems tend to burn with acridity, the acridity is masked or nullified bythe flavoring of smoke from the burning of said tobacco stems withencapsulated odoriferous flavors such as menthol, lime, lemon, peach,pineapple, cherry, spearmint, peppermint and kola.

It has been recognized that the addition of aromatic substances totobacco imparts a pleasant flavor to the tobacco. ln

salvaged and used in the manufacture of smoking articles. Materialsnow'disposed of as waste are tobacco "stems, dust,

scrap, clippings and other portions which are unsatisfactory-inconnection with the manufacture of high-grade smoking articles.

From time to time attempts have been madeto'fQIm-tobacco sheets or filmswhich would solve the problem of satisfactorily disposing of orutilizing tobacco waste -.rnaterials. Processes have beendeveloped forforming tobacco paper 0 utilizing well-known paper processes andtechniques in whieh tobacco waste, such as for example stems and scraps,has been reduced to pulp by the use of chemicals, and then according toordinary paper making techniques converted into paper. These techniquesare unsuitable for use either in connection with the present inventionin forming improved tobacco sheet material, carrying out the processestherefor, and producing novel smoking articles, such as cigarettes orcigars, because of the radical changes to which these tobacco materialsare subjected, and the loss of valuable constituents and properties of 1natural tobacco.

methods hitherto used the tobacco has been treated by soaking it in asuitable solution of the aromatic substance, or the solution has beensprayed on the tobacco. One disadvantage of such a process is that mostaromatic substances which are suitable for this use have an appreciablevapor pressure at ordinary temperatures and forthat reason the substancemore or less rapidly vaporizes andescapes. In the process of theinvention a wide variety of aromatic substances may be used and whenencapsulated in microcapsules the substances do not vaporize and escape.

A means-of overcoming the acridity of reconstituted tobacco sheets madefrom stems of tobacco by including flavor containing capsules on orunder the surface of the sheet material, is to mix the capsules with thepulp prior to the formation of the sheet, or to otherwise generallydistribute the capsules through the body ofthe sheet. With such atechnique in reconstituted tobacco sheet manufacture, the capsules wouldhopefully and at best be distributed throughout the sheet or web.However, efforts to form the sheet material by mixing the capsules andthe tobacco fibers, without more, have been unsatisfactory due to theenormous percentage of escape and loss of capsules through drainage fromthe embryonic reconstituted tobacco sheet or web.

The subject invention provides a system for the penetration in thetobacco industry, and particularly that part of'the industry relating tothe manufacture of cigarettes, cigars and like smoking articles, largequantities of tobacco are rejected annually and sold as waste because itis either impossible or impracticable to utilize them in the manufactureof smoking articles. Obviously the loss of these materials is a seriousmatter from the point of view of the manufacturers and, therefore, itwould be highly desirable if such material could'be According to thisinvention, tobacco sheet or film material may be made along linessimilar to those described and disclosed in U.S. Pat. No. 2,433,877, inwhich thefinal product contains substantially all of the desirableproperties and natu ral characteristics of tobacco, especially insofaras aroma, taste and color are concerned, and has the same generalappearance of tobacco.

Another object .of this invention is to coat reconstituted tobacco sheetmaterial with capsules containing aromatic material such as menthol,lime, lemon, peach, pineapple, cherry, spearmint,'peppermint, and kola.

Another object of this invention is to prevent premature rupture ofcapsules coated on the surface of reconstituted tobacco sheets byproviding a subsident layer of capsules within a reconstituted tobaccosheet such that said subsident capsules are protected from abrasiverupturing forces, in smoking article manufacture, transport, andstorage.

Another object of this invention is to provide flavor containingreconstituted tobacco sheet material in which the flavor is invisibleand undetectable prior to smoking said reconstituted tobacco sheetmaterial. Another object of this invention is to provide a novel methodof making reconstituted tobacco sheet which has the advantage ofphysical protection of capsules containing flavoring from touch andsight. To the 'end that the particles (capsules) may be confined withinthe sheet, they are of necessity much smaller in their average diametersize than the sheet thickness and preferably are of such size, andpresent in such quantity, that they are protectively nested in'theinterstitial spaces between the tobacco fibers of the reconstitutedtobacco support sheet, in addition to being adherent -to the tobaccofiber, even if calendered, without disturbing, from a user's viewpoint,the normal physical structure of such a sheet made without them. I i

The instan-tinvention encompasses the method of forming continuous,self-supportingreconstituted tobacco films or sheets which comprisesforming an aqueous slurry .of comminuted tobacco stems, forming saidslurry into a continuous thin web, and applying to said'web microscopiccapsules each containing an inner phase comprising flavorssuchasmenthol,

' lime, lemompeach, pineapple, cherry, spearmint, peppermint,

and kola, and removing moisture from saidweb.

The tobacco stems, veins, and tobacco leaf'material can be comminuted bymeans of a suitable type-of milhsuch as a ball mill or colloid mill. Anydesired ratio of tobacco material to water canbe used. It has been foundthat ratios of l.8.to l.l4 givesatisfactory results. When the milling orslurry'l'orming operation-is completed, the slurry is deposited ina'fllm forming device and applied in the form ofa continuousfilm or webupon a suitable film forming surface, such that when the slurry isspread out in the form of a film or web thereon,substantially allsoluble and insoluble constituents of the tobacco stems and veins willbe contained in a reconstituted tobacco sheet or film. The tobacco filmcan be coated with encapsulated flavoring material while in either wetor dry condition.

it is not necessary to rupture the capsules contained in a tobaccosmoking article since heat from a burning front of tobacco will rupturethe capsules seriatim thereby releasing aromatic material such that thesmoke emanating from the tobacco smoking article is homogeneouslyflavored.

One of the features of the instant invention is the saving in volatilematerial effected by encapsulation. The evanescence of the volatilematerials is greatly inhibited by the intact capsul wall.

A desirable result obtained by this invention is the formatidn of areconstituted tobacco sheet in which the cross-sectional area ispermanently increased as a result of-the included capsules so that ifcigarettes are formed from this material, either wholly or'fromadmixtures withnatural shredded tobacco, there is a definite increase infilling power of reconstituted capsule-containing material. Due also tothe increased area and decreased thickness of those portions of thesheet or web which contain capsules, the ash formed when this materialis burned approximates more closely the ash of natural tobacco and theodor is more nearly that of natural tobacco although a large portion ofthe tobacco material in the sheet or film consists of stems.

This invention includes the application of one or more other sets ofcapsules throughout the thickness of the reconstituted tobacco sheet oron the outside of the sheet, and it does not preclude the presence ofother material, particulate or other, present in, on the outside of, orotherwise associated with the sheet, to cooperate, or not, with the setof capsules positioned in the sheet by the practice of this inventioncumulatively or countervailing, which produce a beneficial effect. Theremay be two or more sets of capsules in the sheet being confined or notconfined to the surface, or spread throughout the thickness ofthe sheet.

it is contemplated that the embedded particles (capsules) need not beofuniform substance, content, and size. When the particles are capsules,they may be a mixture as to size and wall material or of differentcontent or origin, to serve one or more utilitarian purposes inbehavior, or, if capsules, to have walls of varying resistance torupture or fracture, or to be different in any other aspect of structureor performance (such as resistance to heat) or different in anyolfactory sense characteristics--or to contain chemical reactants,medicines,

perfumes-absorbents r absorbents-as between the fracture and unfracturedstate or'in either stateor to be affected by other forms of energy invarious manners which will be evident to those skilled in the art. Eachof the capsules may be self-contained, in that each, upon rupture,releases its volatile content. The particulate liquid may contain eitherliquid or solid solute material dissolved therein, or have suchmaterials dispersed therein in any physical state, and may containmaterials which may be subject to growth, metamorphosis, ordegeneration.

To obtain disuniformity among capsules if such are used they may bemanufactured in separate batches according to the'characteristies of thecapsules as to origin, size, contents, or \vall'material and structure.and thereafter blended in the desircd'proportions for introduction intothe paper as a single applied slurry. This is important where more thanone kind of capsule contents (solid or fluid) is to be made use ofeither by rupture of the capsules or by their characteristics in theunruptured state. it is within the province of this invention to pro- Icontaining flavoring material intoa reconstituted tobacco sheet as thesheet is being formed, so that the particles are substantiallyconcentrated subsident to either surface thereof in a firm, well definedstratum of binder material.

The capsules are, preferably applied in an aqueous slurry containing asolvent-responsive or solvent-activated adhesive such as a vegetable gumor starch. Efficacious natural adhesives or binders include hydrolyzedstarches (principally tapioca starch), gum arabic, gum tragacanth. Theseadhesives or binders are used exclusively in water solution. (Whilekaraya gum is not actually soluble in water, karaya gum particles absorblarge amounts of water and swell to great size). Certain water solublesynthetic adhesives or binders such as polyvinyl alcohol, sodiumcellulose glycolate. and methyl cellulose can be used to bind capsulesin a reconstituted tobacco web.

The capsules preferably should contain an oily, aromatic liquidcomprising about percent, by weight, of the encapsulated structure. Theoily liquid is released by the rupturing of the capsule wall material.The oily liquid may be a mixture of oils or dispersions of solids inoils. The aggregation of capsules can contain disparate substanceswithin each discrete capsule.

The process of this invention may be employed to form smoking articlescontaining two disparate encapsulated substances which actsynergistically when the capsules containing them are ruptured. Therelative proportions of solid particles to capsules may vary accordingto the effect desired.

The capsule walls can be made of a gelatin-gum arabic complex,gelatin-carrageenan complexes, phased out succinylated gelatins, ethylcellulose, or other material. Any standard method of encapsulation suchas the one set forth in example 1 may be used to form the capsules.

The size of the capsules can range from approximately 5 microns indiameter to approximately 40 microns in diameter. and may be mixed as tosize, or even mixed as to content. Capsules spaced in the cigaretteshould not exceed 40 microns in diameter, since larger capsules tend torupture with a loud report.

Capsules of the 5 to 40 micron size can be made according to the processdisclosed in D5. Pat. No. 2,800,437, which is sued on July 23, 1957 toBarrett K. Green and Lowell Schleicher. Briefly, that patent disclosesfilm-forming polymeric materials of opposite electric charge in aqueoussolution which are caused to form a separate liquid dispersed phase (acoacervate) by modifying the conditions of the solution.

The intended oil contents of the capsules are emulsified in thesolution, and the coaccrvate forms a liquid film about the emulsion. Thefilm is made firm and solid, and is then hardened. The capsules arerecovered ready for their use as part of the heat rupturablecomposition. The oily material of the preferred embodiment (e.g., asolution of menthol) may be replaced in whole or in part by thepreviously mentioned or other materials ofaromatic or therapeuticproperties.

in the accompanying drawings, which illustrate a preferred embodiment ofthe invention, and form a part of this specification, and wherein theseveral reference characters designate the same or like elements:

FIG. I is a diagrammatic view showing mechanism suitable for carryingout and performing the method;

FIG. 2 is a leaf of tobacco having capsules applied to the surfacethereof; I

FIG. 3 is a cross-sectional view of asheet of reconstituted tobaccohaving capsules in a subsident layer therein;

FIG. 4 is a view. of a cigarette made from filler of reconstitutedtobacco containing a subsident layer of capsules each containing aninner phase of aromatic flavoring material;

FIG. 5 is a sectional view of a cigar having a binder formed ofreconstituted tobacco sheet material having a subsident layer ofmicrocapsules each containing an inner phase of aromatic flavoringmaterial, and a composition tobacco filler; and

FIG. 6 is an end view of a cigar in which the tiller consists entirelyof long or short reconstituted tobacco sheet material having a subsidentlayer of capsules each containing an inner phase of aromatic flavoringmaterial.

As mentioned hercinabove, the reconstituted sheet which is made inaccordance with this invention, can be used either in the manufacture ofcigars, cigarettes or other like smoking arminuting machine andpreferably screened to remove any' foreign material such as sand mixedtherewith. The mixture of comminuted stems and leaves is then placed ina ball mill of known design, and ball milled for a period of time,preferably sufficient to completely hydrate or gelatinize the particlesof tobacco being ball milled. The size of the ball mill and balls, andspeed of rotation, control the amount of time necessary to reach thedesired state'of hydration or gelatinization of the tobacco particles.For instance, it has been found that in a 4- gallon jar ball mill using3/4 -inch nominal size flint pebbles, the ball milling time mayapproximate from 6 to 16 hours at 50 rpm. whereas in a S-quart ball millusing the same size pebbles at 60 rpm, the minimum time may run as highas 13 hours.

Upon completion of the slurry, it is removed from the ball mill andplaced in a film forming device and formed into a continuous sheet orweb. The sheet or web material is then ready for the addition ofcapsulesin a slurry.

Mechanism suitable for forming films is shown diagrammatically inFIG. 1. In this mechanism there is provided a conventional type of filmforming unit, designed generally 3, which delivers the sheet material inthe form ofanendless web 4 onto a traveling conveyor 6 running onpulleys 8, 10 mounted on driving and driven shaft l2, 14, respectively.Conveyor 6 preferably is imperforate and is made in the form of anendless band from material, such as stainless steel or other nonrustingand nonstaining material. In this way there is no danger of staining ordiscoloring the sheet or web being formed thereon.

Furthermore, the use ofan imperforate surface substantially prevents theloss of valuable insoluble constituents of tobacco. It will be seen,therefore, that at all stages in the process of making the reconstitutedtobacco sheet care is taken not to lose from the aqueous colloidaldispersion or from the cast sheet films any of the natural solubleingredients or constituents of tobacco and that these solubleconstituents are reincorporated in the finished sheet in substantiallythe proportions in which they occur in the component tobaccos afterevaporation of the excess moisture present in the aqueous hydratedtobacco dispersion.

A primary objective of the invention is to provide processes for makingreconstituted tobacco sheet with limited penetration ofliquid-containing capsules as the particles that, because of theirposition in the sheet, when ruptured by heat, release the containedvolatile flavoring liquid. This objective is accomplished by forming asheet of reconstituted tobacco with the capsules embedded in it. Theamount of capsules applied should be related to the final sheetthickness and the amount ofencapsulated liquid necessary or desirable tobe provided.

Considering now the application of the subject invention to theproduction of sheet material, the preferred system comprises laying downa wet web of tobacco fibrous material on a supporting member to form anembryonic sheet, and applying to said web minute capsules, the contentsof which capsules comprise flavoring material.

Following the formation of the sheet or web, it is moved through amoisture removing zone and excess moisture is removed therefrom. In FIG.I there is shown a hood, designated generally 16 through which hot aircan be delivered against the surface of the web or sheet material toremove the .desired amount of moisture therefrom. This may be all oronly-a part depending upon the condition of the sheet or web.

it should be understood that the foregoing description of FIG. I ismerely illustrative. it is within the scope of this invention to add thecapsules by any means at any point in the tobacco web formation providedthat the web at the time of addition of the capsules 2! is sufficiently\vet and penetrable, either by reason of undrained liquid or because thecapsular particulate material was added as a liquid slurry, to permitfixation on the tobacco fibers. Thus, while the preferred procedure, asshown in FIG. 1, calls for the addition of the capsules 21 at 22,thecapsular slurry might be added at another point, again provided thatthe web of tobacco sheet material allowed sufficient penetration of thecapsular material into the tobacco web.

Following are examples of systems that produce a controlled penetrationof capsules within a reconstituted tobacco sheet or web.

EXAMPLE I of the invention as carried out using the process steps andapparatus shown in FIG. 1, wherein minute capsules were added to a wetweb of reconstituted tobacco. The capsules and binder materials, whenplaced among the tobacco'fibers, wet them and entangle with them andclothe them, thus in effect securing and binding the capsules againstmigration through the sheet, thereby forming a subsident stratum. Themajority of binder and associated capsules are caught in the sheet.Substantially no capsules migrate through the sheet. When the wettobacco web is dried, the binder shrinks by loss of solvent, leaving thedried polymeric binder material, and the capsules remain in placerelatively with respect to sheet thickness. The apparatus and theprocedure for adding the components were as shown in FIG. 1.

Tragacanth gum solution and starch solution were prepared in thefollowing manner:

Concentrated Tragacanth Gum Solution Four and five-tenths pounds of drytragacanth gum powder was stirred into 50 gallons of water, using asuitable mixer.

Five minutesafter all the powder had been added, the mixer combining thetragacanth gum solution and the capsular slurry, 50 gallons oftragacanth gum solution was diluted with water to 3 percent tragacanthgum on a solids basis.

Starch Solution The hydrolyzed starch solution was prepared by heating aslurry of the starch at F. for a minimum of l5 minutes to provide a lpercent-by weight, starch-in-watcr solution.

Preparation ofCapsular Slurry Encapsulation of Lemon Oil Ten grams ofgum arabic were dissolved at room temperature in 200.0 grams ofdeionized water. The mixture was agitated until the gum arabic was fullydissolved. In a separate 250 milliliter Erlenmeyer flask, 10.0 grams ofmodified gelatin was mixed with 200.0 grams of deionized water. Thegelatin was allowed to'tumcfy at room temperature and also then warmedin a water bath to about 40C. with stirring so that the gelatin wasdissolved.

The gelatin solution and the gum arabic solution were poured into abeaker equipped with a stirrer. A flocculence indicating theprecipitation of the gelatin was noted. The temperature of the mixturewas decreased to 35C. The speed of the stirrer was adjusted so that itwas turning only enough to keep the phases mixed. The pH of the mixturewas 4.2.

Into the beaker containing the mixture of gum arabic and gelatin waspoured 1 18.0 grams of lemon oil. The speed ofthe stirrer was thenadjusted to mix the colloids and the oil. The oil separated intodroplets. Two drops of octyl alcohol were added to prevent foaming. Theprogress of the coacervation was monitered by means of microscopicexamination.

The temperature of the mixture was lowered to room temperature, i.e.,24C. At the higher temperature of 31C. colloid deposition was observedon the oil droplets. At 24C. little colloid could be observed in aqueousportions of the mixture. Deposition had ceased. Stirring was continuedfor 30 minutes, whereupon the reaction mixture was cooled on an ice bathto 4C. The reaction mixture was maintained at this temperature for 200minutes. (When hardening was desired, 1,0 milliliters of a 25 percentglutaraldehyde in water per gram of gelatin is added.)

After stirring, a mass of capsules thus formed were refrigerated to 4C.and maintained at that temperature for a time interval of 12 to 16hours. After refrigeration, the cold capsule mass was placed in aseparatory funnel and undeposited colloid material allowed to separateto the bottom of the vessel whereupon it was withdrawn and discarded.The drying of the capsules formed supra was effected by first rinsingthe capsules with cyclohexane. The cyclohexane was decanted. Thirteenand three-tenths grams of finely divided hydrated calcium silicate wasmixed with cold deionized water to form a thick, mobile slurry. Theslurry thus formed was stirred into the mass of capsules. Cold deionizedwater was added as needed to form a viscous, yet fluid base. The pastethus formed was poured into a Buchner funnel and vacuum filtered; thetop of the funnel being sealed with a sheet of rubber. When no furtherwater was observed being compressed from a filter cake thus formed, thefilter cake was placed on a clean, absorbent paper and allowed to dryunder ambient laboratory conditions.

An alternative drying method comprises adding 200.0 grams of coldhexylene glycol for each 100.0 grams of moist, rinsed, capsules. Thecapsules are mixed with the hexylene glycol. The hexylene glycol isdrained from the capsules through the pores of a 200 mesh sieve. Theforegoing was repeated twice. After the third and final rinse, however,the hexylene glycol was removed by Buchner funnel filtration. After thefiltration was complete, the capsules were placed on a clean, absorbentpaper and dried at ambient laboratory temperature.

The internal phase of the capsules thus formed was approximately 80-90percent ofthe total weight of the capsules.

Variation of the Encapsulation of Lemon Oil to room temperature and thenfurther decreased to a temperature of 4 to 10C. by means of an ice bath.The capsules thus formed were dried in the procedure set forth above.

Encapsulation of Kola Flavor The procedure for the encapsulation oflemon oil, set forth supra, was followed-except that the inner phase waskola flavor, the droplet size of said kola flavor being 10 microns. Thehardening agent for the capsule walls was a -percent solution ofglutaraldehyde in water.

A further aspect of the subject invention concerns the nature of thefibrous tobacco sheet material resulting from carrying out the processof this invention. The sheet of the invention differs from earlierfibrous sheets in that the penetration of the particulate material issubstantially uniform. In the usual fibrous sheet, though attempts aremade to achieve a uniform laydown of fiber, this is generally difficultto obtain. and, for this reason, penetration of capsules in a uniformstratum is impossible of attainment without the agency of thisinvention. 1n the subject invention, it has been found that the capsulespenetrate over the area applied, to a substantially uniform degreethrough a thickness of the tobacco web to form a subsident layertherein.

Referring again to FIG. 1, shaft 12 can be driven continuously at a rateof speed required to remove either all or only a part ofthe moisturecontained in the web.

Obviously conveyor 6 can be driven stepwise ifdesired. The partiallydried web or sheet material is delivered by conveyor 6 onto conveyor 15which in the embodiment selected for purposes of illustration is also anendless band consisting preferably of stainless steel or other heatresistant material. Conveyor 15 runs upon pulleys l7, 19 mounted onshafts 26, 28. Shaft 28 is driven in timed relation with driving shaft12 so that the movements of the conveyors 6 and 15 are at the same rateof speed. It is preferred that the movement ofconveyors 6 and 15 becontinuous because it is believed that it results in a more efficienthandling of the web or sheet material being treated. in this manner theweb material 4 advancing past the capsule addition 22 is graduallyheated.

The speed of conveyor 15 is governed in part by the thickness andmoisture content of web 4. If a web is, say onethousandth of an inch inthickness and contains say S-percent moisture, it is necessary to runconveyor 15 faster than when the web being treated is, sayfour-thousandths of an inch thick and contains the same amount ofmoisture. Speed of conveyors 6 and 15 is thereby adjusted in accordancewith web thickness and moisture content. lf conveyor 15 is driven at afaster rate of speed than conveyor'6, provisions can be made in anyknown manner for controlling movement of web 4 from one conveyor to theother. lt is also necessary to take into consideration the temperatureand proximity of heat source to the web.

As the capsule containing sheet material 5 is moved by conveyor 15 fromthe heat treating zone, lengths are cut therefrom by a cutting mechanismconsisting of a rotary knife 23, and coating roller 27 operated in timedrelationship with the movement of conveyor 15. The lengths can then bepacked for storage or they may be used in the formation of cigar filleror binders. 1f the capsule-containing tobacco sheet material is to beused as a cigarette tobacco filler, it can be shredded by any knownmeans and added in desirable quantities to form a desired cigarettetobacco blend.

FIG. 2 shows a tobacco leaf with capsules 21 adherent to the surfacethereof.

HO. 3 disclosed a cross-sectional view of a sheet of reconstitutedtobacco S containing capsules 2] and tobacco materi- FIG. 4 discloses acigarette designated generally 40, in which the conventional wrapper 42encloses a filler consisting of shreddedcigarette tobacco 44 andshredded capsule containing reconstituted tobacco filler material 46. orcapsule containing reconstituted tobacco filaments 46 in any desiredproportion. lt is evident that the tobacco film or filaments can be madefrom various types and combinations of tobacco. For instance, thetobacco sheet material can be made from relatively expensive tobaccosuch as Latakia in which it is highly desirous to use all waste becauseof the high price thereof. So, also, it may be formed ofBurley or one ormore scrap or waste cigarette-type tobaccos and incorporated inaccordance with a particular cigarette manufacturers formula as if itwere natural cigarette tobacco leaves. Any desired formula can thus bemaintained in accordance with the demands of a manufacturers particularbrand using one or more types of natural shredded tobacco leaves andadmixed desired quantities of shredded capsule containing tobacco filmmaterial or filaments, either as a blending or flavoring medium or bothor for purposes of bulking.

H6. shows a representation of a cigar 50, which may be a long or shortfiller cigar depending upon the kind of filler used. Cigar 50 has awrapper 52, a binder 54 formed from capsule containing tobacco sheet orfilm material and a composite filler consisting of long or short fillertobacco 56, and a desired quantity of pieces of capsule containingtobacco sheet material or film 58 of desired size employed for blendingand/or bulking or natural tobacco filler 56 alone. The amount of capsulecontaining tobacco used depends upon the types of tobacco employed inmaking the reconstituted tobacco sheet. and the requirements of aparticular blend. If desired, instead of a binder formed of tobacco filmmaterial, such as 58, a conventional type of tobacco leaf binder may beused. FIG. 6 shows a cigar in which the filler consists entirely of longor short filler reconstituted tobacco sheet material containing capsules60, and a natural leafbinder 62.

The invention above described may be varied in construction within thescope of the claims, for the particular device,

selected to illustrate the invention, is but one ofmany possibleconcrete embodiments of the same. It isnot therefore to be restricted tothe precise details of the structure shown and described.

EXAMPLE Encapsulation of Menthol Three-thousand seven-hundred and fiftycubic centimeters of a (SO-percent of solution of oil of menthol inwater and 297 grants of gelatin in 5,403 cubic centimeters of water wasstirred in a dispersator until the particle size was in the range of 5microns to 40 microns (75 minutes stirring). A solution of 297 grams ofgum arabic' in 5,403 cubic centimeters of deionized water was thenadded. The pH of the resulting mixture was adjusted to 4.8 by theaddition of a lO-percent solution of sodium hydroxide in water.Six-thousand cubic centimeters of water was added at a temperature of38C. The mixture was slowly cooled on awater bath to a temperature of38C. One-hundred and forty-eight and five-tenths cubic centimeters of a'25-percent solution of glutaraldehyde in water was added. Approximatelyl gram of gelatin (additional) was added and the resulting mixture wasstirred for 12 hours. Seven and seventenths grams of methylparahydroxybenzoate was added. The resulting capsule slurry was stirredfor 30 minutes and then filtered using a No. 30 sieve.

The capsule mass was allowed to stand until the capsules can be decantedfrom the excess colloid. The capsules were washed twice with colddeionized water and that colloidal material separating from the capsulesbeing decanted.

A slurry was prepared by mixing 400 parts by weight of fine ly dividedhydrated silica in 250.0 parts by weight of deionized water. Thecapsules were suspended in the slurry, then the slurry mass was filteredover a Buchner filter. The resultant filter cake was broken up andallowed to dry for 24 hours.

The capsules were suspended in a mixture of 3 parts gum tragacanth and97 parts water and the resulting suspension was sprayed on tobaccoleaves. (See FIG. 2).

EXAMPLE III Encapsulation of Menthol-Peppermint Oil Slurry Eighteenparts by weight of spray dried gum arabic was dissolved in 384.5 partsby weight of deionized water in a beaker equipped with a stirrer. In aseparate 250 milliliter Erlenmeyer flask, 18.0 parts by weight ofgelatin was dissolved in 384.5 parts by weight ofdeionized water.

Fifty-eight and five-tenths parts by weight of menthol crystals andl36.5 parts by weight of peppermint oil were added to the gum arabicsolution. The temperature of the mixture was adjusted to 33C.Thereafter, the solution of gelatin was added with rapid stirring. Thereaction mixture was cooled to a temperature of 10C. on an ice bathwhile continuously stirred. The-mixture was stirred for one hour at l0C.Thereafter, 18.0 parts by weight of a 25-percent solution ofglutaraldehyde in water was added to the reaction mass.

The reactant mass was stirred at l0C. for 8 hours. The capsules thusformed were dried in the manner set forth in example II. The capsuleswhich were sprayed onto cut tobacco leaves exhibited an inner phase ofmenthol-peppermint oil slurry.

EXAMPLE IV The procedure of example ll was followed except that the-menthol was substituted with a menthol-methane slurry.

The mixture in the inner phase of the capsules was comprised of l36.5parts by weight of menthol crystals and 58.5 parts by weight menthone.

EXAMPLE V The procedure of example ll was followed except that thementhol of example ll was substituted with a menthol-peppermint slurry.

EXAMPLE VI The procedure of example ll was followedexcept that spearmintoil was substituted for the menthol oil of example II.

EXAMPLE VII The procedure of example ll was followed except that a limeoil was substituted for the menthol oil of example ll.

The solution for the inner phase was comprised of l95.0 parts by weightlime oil and 0.975 parts by weight butylated hydroxy anisole.

In the case of the manufacture of cigarettes, according to the presentinvention, tobacco films are shredded into strands or the film is formeddirectly into filaments substantially the width of the strands ofnatural shredded tobacco and of any desired length, in the case ofcigars, the capsule-containing films are used in large pieces much aslong filler tobacco in forming long filler cigars or in smaller piecesfor use in the formation of short filler cigars. in all cases theshredded films or filaments or film used in cigarettes and cigars can behandled either manually or by machine in the same manner as naturalshredded tobacco leaves or whole leaves or portions thereof. The amountof shredded capsule-containing reconstituted tobacco or pieces of thismaterial employed in a particular blend in cigarettes or cigars,respectively, will vary according to types of tobacco used in the sheetmaterial and the requirements of a particular manufacturer.

We claim: v

1. A method of forming continuous self-supporting reconstituted tobaccosheets which comprises comminuting tobacco stems and tobacco leaves,forming an aqueous slurry from said comminuted tobacco stems and tobaccoleaves. forming said slurry into a continuous web, adding an aqueousslurry of tragacanth gum and a plurality of minute rigid-walled,heatrupturable capsules, each containing an inner phase of a flavoringmaterial, said capsules having an average diameter smaller than thethickness of the sheet and preferably of such size and in. such quantitythat they are protectively nested in the interstitial spaces between thetobacco fibers, and removing moisture from said web.

2. A process for limiting the penetration of microcapsules through anembryonic reconstituted tobacco sheet, comprising forming a wet web offibrous tobacco on a suitable support member, said wet tobacco web beingsufficiently free to allow drainage of liquid and passage ofmicrocapsules'thereinto, and applying a plurality of microcapsules inthe form of a liquid suspension to said wet web, said microcapsuleshaving an average diameter smaller than the thickness of the sheet andmaterial envelopes the said capsules and simultaneously adheres to theproximate tobacco fibers, thereby to affix said capsules to tobaccofibers.

